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WO2002101773A1 - Solution electrolytique pour condensateur electrolytique et condensateur electrolytique utilisant cette solution - Google Patents

Solution electrolytique pour condensateur electrolytique et condensateur electrolytique utilisant cette solution Download PDF

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Publication number
WO2002101773A1
WO2002101773A1 PCT/JP2002/004571 JP0204571W WO02101773A1 WO 2002101773 A1 WO2002101773 A1 WO 2002101773A1 JP 0204571 W JP0204571 W JP 0204571W WO 02101773 A1 WO02101773 A1 WO 02101773A1
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WIPO (PCT)
Prior art keywords
electrolytic solution
solvent
electrolytic capacitor
electrolytic
capacitor according
Prior art date
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PCT/JP2002/004571
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English (en)
Japanese (ja)
Inventor
Masayuki Takeda
Masahiro Takehara
Makoto Ue
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Mitsubishi Chemical Corporation
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mitsubishi Chemical Corporation filed Critical Mitsubishi Chemical Corporation
Priority to EP02778902A priority Critical patent/EP1394824A4/fr
Priority to CNB028097165A priority patent/CN100394522C/zh
Publication of WO2002101773A1 publication Critical patent/WO2002101773A1/fr
Priority to US10/704,803 priority patent/US7072173B2/en
Priority to US11/304,600 priority patent/US7460357B2/en

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/022—Electrolytes; Absorbents
    • H01G9/035—Liquid electrolytes, e.g. impregnating materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/08—Housing; Encapsulation
    • H01G9/10—Sealing, e.g. of lead-in wires
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/145—Liquid electrolytic capacitors

Definitions

  • the present invention relates to an electrolytic solution for an electrolytic capacitor and an electrolytic capacitor using the same.
  • Electrolytic capacitors are characterized by having a large capacitance while being small, and are frequently used for low-frequency filters and bypasses.
  • An electrolytic capacitor generally has a structure in which an anode foil and a cathode box are wound through a separator, and this is housed in a case and sealed (see FIGS. 1 and 2).
  • Metal such as aluminum or tantalum having an insulating oxide film formed as a dielectric layer is used for the anode foil, and an etched aluminum foil is generally used for the cathode foil.
  • the separator interposed between the anode and the cathode is impregnated with electrolyte to prevent a short circuit between the two electrodes, and functions as a true cathode.
  • electrolyte is an important component that has a significant effect on the characteristics of electrolytic capacitors.
  • the electrical conductivity is directly related to the energy loss impedance property of the electrolytic capacitor and the like, and therefore, the development of an electrolyte having a high electrical conductivity is actively performed.
  • a quaternary ammonium salt such as phthalic acid / maleic acid (Japanese Patent Application Laid-Open No.
  • Electrolyte solutions for electrolytic capacitors are required to have higher electrical conductivity, better thermal stability, and higher withstand voltage properties, and also to have these properties. Electrolytic capacitors are also required to have lower impedance, better thermal stability, and higher withstand voltage, and to have both of these properties. However, heretofore, the electrolytic solution for electrolytic capacitors and
  • the present invention (1) is an electrolyte for electrolytic capacitor containing tetrafluoropropoxy O lower Rumin acid ion, a tetra full O lower Rumin acid ion, quaternary Oniumu salt Tet rough Ruo lower Rumin acid
  • the electrolytic solution for an electrolytic capacitor described above which is contained in the form of one or more salts selected from the group consisting of an amine salt, an ammonium salt, and an alkali metal salt.
  • the present invention is an electrolytic capacitor using the electrolytic solution for an electrolytic capacitor of the present invention (1), and is an electrochemical device using a conductive material containing tetrafluoroaluminate ion.
  • the present invention (2) is an electrolytic solution for an electrolytic capacitor containing a salt and a solvent, wherein the electric conductivity X (mS-cm " 1 ) at 25 ° C and the withstand voltage Y (V) of the capacitor are: Equation (I):
  • the present invention provides an electrolytic solution comprising: a solvent containing 50% by weight or more of a solvent, a boiling point in the solvent of 250 ° C. or more, a melting point of 60 to 40 ° (: and a dielectric constant ( ⁇ , 25 ° C.
  • the weight ratio of the solvent having a boiling point of at least 190, the boiling point of less than 250 ° C, the melting point of 1 to 40 ° C, and the dielectric constant ( ⁇ , 25 ° C) of 25 or more The electrolytic solution for an electrolytic capacitor of the present invention (2), wherein the electrolytic solution contains a solvent in an amount of 50% by weight or more, and has a boiling point in the solvent of 190C or more, less than 250 ° C, and a melting point of 60 to 40.
  • the weight ratio of the solvent having 25 or more is boiling point 250 ° C or more, melting point-60 to 40 ° C, and dielectric constant ( ⁇ , 25 ° C)
  • the electrolytic solution for electrolytic capacitors according to the present invention (2) which exceeds the weight ratio of the solvent having 25 or more.
  • the present invention is an electrolytic capacitor using the electrolytic solution for an electrolytic capacitor of the present invention (2).
  • FIG. 1 is a perspective view of a wound type element of an electrolytic capacitor, wherein reference numeral 1 denotes an anode foil, reference numeral 2 denotes a cathode foil, reference numeral 3 denotes a separator, and reference numeral 4 denotes a lead wire.
  • FIG. 2 is a cross-sectional view of the electrolytic capacitor.
  • Reference numeral 5 denotes a sealing material, and reference numeral 6 denotes an outer case.
  • FIG. 3 is a graph showing the relationship between the electric conductivity X of the electrolytic solution for an electrolytic capacitor of the present invention and the withstand voltage Y of the electrolytic capacitor.
  • a first aspect of the present invention is an electrolytic solution for an electrolytic capacitor containing tetrafluoroaluminate ions.
  • Anion component in electrolyte for electrolytic capacitor thus, it has been found that when tetrafluoroaluminate ions are contained, an electrolytic solution having high electric conductivity, excellent thermal stability, and high withstand voltage can be obtained.
  • the tetra.fluoroaluminate ion is a monovalent anion formed by bonding four fluorine atoms to an aluminum atom, represented by the chemical formula: A 1 F 4 —, and is also referred to as tetrafluoroaluminate. .
  • tetrafluoroaluminate ions are used for all or a part of the anion component, and the tetrafluoroaluminate ion in the anion component is preferably 5 to 100 mol%. It is preferably from 30 to 100 mol%, particularly preferably from 50 to: 100 mol%, most preferably 100 mol%.
  • the electrolytic solution of the present invention may contain tetrafluoroaluminate ion in the form of a salt in the electrolytic solution.
  • the tetrafluoroaluminate is preferably at least one selected from the group consisting of quaternary ammonium salts, amine salts, ammonium salts and alkali metal salts.
  • quaternary ammonium salt examples include a quaternary ammonium salt, a quaternary phosphonium salt, a quaternary imidazolyme salt and a quaternary amidinium salt.
  • quaternary ammonium ion of the quaternary ammonium salt include the following.
  • tetramethylammonium methyltrimethylammonium, methyldimethylammonium, triethylmethylammonium, tetraethylammonium, trimethyl_n-propylammonium, trimethylisopropylammonium , Trimethyl-n-butylammonium, trimethylisobutylammonium, trimethyl-t-butylammonium, trimethyl n-hexylammonium, dimethyldi-n-propylammonium, dimethyldiisopropylammonium, Dimethyl-n-propyl isopropyl ammonium, methyl tri-n-propyl ammonium, methyl triiso Propylammonium, Methyldi-n-propylisopropylammonium, Methyl-n-propyldisopropylammonium, Triethyl n-propylammonium, Triethyliso
  • Aromatic substituted ammonium For example, those having a total of 4 to 12 carbon atoms, such as trimethylphenylammonium, and those having a total of 13 or more carbon atoms, such as tetraphenylammonium.
  • pyrrolidiniums such as N, N-dimethylpyrrolidinium, N-ethyl-N-methylpyrrolidinium, N, N-getylpyrrolidinium, N, N-tetramethylenepyrrolidinium; N, N-dimethylbiberidinium Piberidinium, such as aluminum, N-ethyl-N-methylbiperidinium, N, N-getylpiperidinium, N, N-tetramethylenepiperidinium, N, N-pentamethylenepiperidinium Morpholiniums such as N, N-dimethylmorpholinium, N-ethyl-N-methylmorpholinium, and N, N-getylmorpholinium. All of these have a total of 4 to 12 carbon atoms. However, the electrolyte solution of the present invention may have a total of 13 or more carbon atoms.
  • pyridinium such as N-methylpyridinium, N-ethylpyridinium, Nn-n-propylpyridinium, N-isopropylpyridinium, N-n-butylpyridinium and the like can be mentioned. . All of these have a total of 4 to 12 carbon atoms, but those having a total of 13 or more carbon atoms can be used for the electrolytic solution of the present invention.
  • the quaternary phosphonium ion of the quaternary phosphonium salt include tetramethylphosphonium, triethylmethylphosphonium, tetraethylphosphonium and the like. All of these have a total of 4 to 12 carbon atoms, but those having a total of 13 or more carbon atoms can be used in the electrolytic solution of the present invention.
  • quaternary imidazolym ion of the quaternary imidazolyl salt examples include 1,3-dimethylimidazolym, 1,2,3, -trimethylimidazolym, and 1-ethyl-3-methylimidazolym.
  • a quaternary imidazonium having a total of 13 or more carbon atoms can also be used.
  • 1,3-dimethyl-2-n-decenylimidazo And dimethyl-1,21-heptanyldecyl imidazolium can also be used in the electrolytic solution of the present invention.
  • 2- (2′-hydroxy) ethyl-1,3-dimethylethyl Midazolym 1- (2'-hydroxy) ethyl-2,31-dimethylimidazolym, 21-ethoxymethyl-1'3-dimethylimidazolym, 1-ethoxymethyl-2,3-dimethylimidazolium and the like.
  • Preferred examples of the quaternary amidinium include 1,3-dimethylimidazolidinum, 1,2,3—trimethylimidazolidinum, 1-ethyl-3, -methylimidazolinium, 1-ethyl-2, 3—Dimethylimidazolidinum, 1, 3—Jetylimidazolidinum, 1,2-Jetyl—3—Methylimidazolidinum, 1, 3—Jetyl-2-methylimidazolidinum, 1 , 2-Dimethyl-3-n-propylimidazolinium, 1 n-butyl-3-methyl Imidazolinium, 1-methyl-3-n-propyl-1,2,4-dimethylimidazolinium, 1,2,3,4-tetramethylimidazolinium, 2-ethyl-1,3-dimethylimidazonium, 1,3-dimethyl-1-n-propylimidazolinium, 1,3-dimethyl-2-n-pentylimidazolid
  • Imidazoliniums such as 1,3-dimethylimidazolinium; 1,3-dimethyltetrahydropyrimidinium, 1,3-getyltetrahydropyrimidinium, 1-ethyl-13-methyltetrahydropyrimidinium , 1,2,3-trimethyltetrahydropyrimidinium, 1,2,3-triethyltetrahydropyrimidinium, 1-ethyl-2,3-dimethyltetrahydropyrimidinium, 2-ethyl-1, 3—Dimethyltetrahydropyrimidinium, 1,2-Getyl-3-Methyltetrahydropyrimidinium, 1,3-Getyl-2-methyltetrahydropyrimidinium, 5-Methyl-1,5-diazabicyclo [4.3.0] nonedium-5,8-methyl-1,8-diazabicyclo4.0] tetracenepyrimidinium such as 7 .
  • a quaternary amidinium having a total of 13 or more carbon atoms can also be used.
  • 1,3-dimethyl-2-n-didecylimidazolyl is preferable.
  • a quaternary amidinium containing a hydroxyl group or an ether group can also be used in the electrolytic solution of the present invention.
  • 2- (2′-hydroxy) ethyl-1,3-dimethylethyl Midazodium 1- (2'-hydroxy) ethyl 1,2,3-dimethylimid Dazolinium, 2-ethoxymethyl-1,3-dimethylimidazolidinum, 1-ethoxymethyl-2,3-dimethylimidazolidinum and the like can be mentioned.
  • the electrolytic solution of the present invention may contain, in addition to the quaternary ammonium salt, an amine salt, an ammonium salt (NH 4 + A 1 F 4 —), and a tetrafluoroaluminate ion as an alkali metal salt.
  • Preferred examples of the amine of the amine salt include trimethylamine, ethyldimethylamine, getylmethylamine, triethylamine, pyridine, N-methylimidazole, 1,5-diazabicyclo [4.3.0] nonene-5, 1,8-Diazabicyclo [5.4.0] tertiary amines such as pendene-7.
  • tertiary amines such as pendene-7.
  • primary amines and secondary amines can be used. For example, getylamine, diisopropylamine, isoptylamine, di-2-amine!
  • Tylhexylamine, pyrrolidine, piberidine, morpholine, hexamethyleneimine, ethylamine, n-propylamine, isopropylamine, t-butylamine, sec-butylamine, 2-ethylhexylamine, 3-methoxypropylamine, 3-ethoxypropylamine and the like can be mentioned.
  • the alkali metal include lithium, sodium, potassium, rubidium, and cesium.
  • quaternary monomer having a total carbon number of 4 to 12 is preferred, and among them, tetraethylammonium is preferred.
  • Triethylmethylammonium getyldimethylammonium, ethyltrimethylammonium, tetramethylammonium, N, N-dimethylpyrrolidinium, N-ethyl-N-methylpyrrolidium, 1,3-dimethyl 1,2-, 3-trimethylimidazolime, 1-ethyl-3, -methylimidazolime, 1-ethyl-2,3-dimethylimidazolime, 1,2,3,4-tetramethylimidazolime, 1 , 3—Jetylimidazolium, 2-Ethyl—1,3—Dimethylimidazolium, 1,3-Dimethyl-2-n—propylimidazolium, 1,3— Methyl-2-n-pentylimidazolym, 1,3-dimethyl-2-n-butylimidazolium, 1,3,4-trimethylimidazolym, 2-ethyl-1,3,4-1 Trimethylimid
  • the electrolytic solution of the present invention may contain an anion component other than tetrafluoroaluminate ion.
  • the salt hydrogen phthalate, hydrogen maleate and the like can be used in combination.
  • tetrafluoroaluminate when used in combination with hydrogen fluoride, hydrogen maleate, or the like, it is preferable that tetrafluoroaluminate is mainly used, and tetrafluoroaluminate is used based on the total weight of the salt.
  • the content of loaluminate is preferably 50% by weight or more, more preferably 60% by weight or more, and even more preferably 70% by weight or more. The higher the ratio, the more preferable.
  • the tetrafluoroaluminate of the present invention When used for an electrolytic capacitor, it must be of high purity, so the salt is used after being purified to the desired purity by recrystallization, solvent extraction, or the like, if necessary. You.
  • the concentration of the tetrafluoroaluminate is preferably 5 to 40% by weight, more preferably 10 to 35% by weight. This is because if the concentration is too low, the electric conductivity is low, and if the concentration is too high, the viscosity of the electrolytic solution increases, and salt precipitation at low temperatures tends to occur.
  • the withstand voltage of the electrolytic solution for electrolytic capacitors tends to increase as the concentration decreases, so that the optimum concentration can be determined by the rated voltage of the desired capacitor.
  • the electrolytic solution of the present invention may be a concentrated solution containing 50% or more of a salt or a room temperature molten salt.
  • the electrolytic solution of the present invention preferably contains 50% by weight or more of a solvent from the viewpoint of obtaining an electrolytic solution having more excellent electric conductivity, thermal stability, and withstand voltage.
  • the solvent includes at least one selected from the group consisting of carbonate, carboxylate, phosphate, nitrile, amide, sulfone, alcohol, and water. Tend to exhibit stable characteristics It is preferable to select from carbonate, carboxylate, phosphate, nitrile, amide, sulfone and alcohol. When water is used as the solvent, it is preferable to use it as a part of the solvent in combination with another solvent.
  • Chain ester carbonates eg, chain carbonates such as dimethyl carbonate, ethyl methyl carbonate, getyl carbonate, diphenyl carbonate, methyl phenyl carbonate, etc.
  • cyclic carbonates eg, ethylene carbonate, propylene carbonate, 2,3-dimethyl ethylene carbonate
  • Carbonic acid esters such as butylene carbonate, pinylene carbonate, cyclic ester carbonates such as 2-vinylethylene carbonate; aliphatic carboxylic acid esters (eg, methyl formate, methyl acetate, methyl propionate, ethyl acetate, propyl acetate, butyl acetate) Amyl acetate, etc.), aromatic carboxylic acid esters (eg, aromatic carboxylic acid esters such as benzoic acid meter, benzoic acid ethyl, etc.), lactones (eg, ⁇ - butyrolactone, r
  • a non-aqueous solvent in which the solvent has a relative dielectric constant ( ⁇ , 25 ° C.) of 25 or more can be preferably used.
  • a non-aqueous solvent in which the solvent has a flash point of 70 ° C. or higher can also be preferably used.
  • the solvent must have a boiling point of 250 ° C or more, a melting point of 60 to 40 ° C, and a dielectric constant ( ⁇ , 25 ° C) of 25 or more.
  • the solvent is preferably contained in an amount of at least 25% by weight, more preferably at least 40% by weight, particularly preferably at least 50% by weight, based on the total weight of the solvent.
  • examples of such a solvent include sulfone, and sulfolane and 3-methylsulfolane are particularly preferable.
  • the solvent has a boiling point of 190 or more, less than 250, a melting point of 60 to 40 ° C, and a dielectric constant ( ⁇ , 25 ° C).
  • the solvent is preferably 25% by weight or more, more preferably 40% by weight or more, and particularly preferably 50% by weight or more, based on the total weight of the solvent.
  • examples of such a solvent include a carbonate, a sulfonic acid ester, a phosphate, a nitrile, an amide and an alcohol, and particularly preferred are carboxylactone and ethylene glycol.
  • the solvent is sulfolane from the viewpoint of thermal stability, and tetrafluoroaluminate 1,1-ethyl-2,3-dimethylimidazolinium or tetrafluoroaluminate 1,2,3 Electrolyte electrolyte solution in which 1,4-tetramethylimidazonium is added in an amount of 5 to 40% by weight based on the total weight of the electrolyte solution.
  • the solvent is arptyrolactone, and tetrafluoroaluminic acid 1-Ethyl 2,3-dimethylimidazolinium or 1,2,3,4-tetramethylimidazolinium tetrafluoroaluminate 5 to 40% by weight based on the total weight of the electrolyte % Electrolytic solution for electrolytic capacitors.
  • a solvent using a combination of sulfolane and arptyrolactone is also preferable.
  • additives other than salts and solvents may be used in the electrolyte solution of the present invention.
  • the purpose of adding additives to the electrolyte solution is wide-ranging, such as improving electrical conductivity, improving thermal stability, suppressing electrode deterioration due to hydration or dissolution, suppressing gas generation, improving withstand voltage, improving wettability, etc. Can be mentioned.
  • the content of the additive is not particularly limited, but is preferably in the range of 0.1 to 20% by weight, and more preferably in the range of 0.5 to 10% by weight.
  • additives include nitro compounds such as p-ditrophenol, m-nitroacetophenone, and p-nitrobenzoic acid; dibutyl phosphate, monobutyl phosphate, dioctyl phosphate, monooctyl octylphosphonate, phosphoric acid, and the like.
  • Phosphorus compounds Phosphorus compounds; Boron compounds such as complex compounds of boric acid and polyhydric alcohols (ethylene glycol, glycerol, mannitol, polyvinyl alcohol, etc.); Metal oxide fine particles such as silica and aluminosilicate; Polyethylene glycol And polyalkylene glycols such as polypropylene glycol and copolymers thereof, and surfactants such as silicone oil.
  • the electrolytic solution of the present invention may be solidified by adding a polymer compound thereto, and used as a so-called gelled electrolytic solution.
  • the polymer used in such a gelling electrolyte include polyethylene oxide, polyacrylonitrile, polytetrafluoroethylene, polyvinylidene fluoride, polymethyl methacrylate, and the like.
  • the life characteristics of a capacitor using such an electrolytic solution are more stabilized by controlling the water content.
  • a non-aqueous solvent used as the solvent of the electrolytic solution
  • the anode and cathode elements undergo hydration degradation during long-term use, and gas is generated at the same time. It is known.
  • the chemical conversion property when repairing the anodic oxide film tends to be poor. It is also known to have a direction.
  • the capacitor using the electrolytic solution of the present invention can be used in a high voltage range up to the rated voltage of 100 V class and also satisfies the requirement of high heat resistance. Unlikely, the effect of water content is significant.
  • the water concentration in the electrolytic solution is preferably 1% by weight or less, and preferably 0.0 in consideration of the above-described chemical conversion. It is from 1 to 1% by weight, particularly preferably from 0.01 to 0.1% by weight.
  • the present invention also provides an electrolytic capacitor using the electrolytic solution according to the present invention.
  • electrolytic capacitors include aluminum electrolytic capacitors, tantalum electrolytic capacitors, and niobium electrolytic capacitors.
  • the structure and material of the electrolytic capacitor are not particularly limited as long as the electrolytic solution according to the present invention is used. Therefore, any use of the electrolytic solution of the present invention for a conventionally used electrolytic capacitor or a newly proposed electrolytic capacitor is included in the scope of the present invention.
  • an element formed by winding an anode foil and a cathode foil via a separator paper is used.
  • anode foil a 99.9% pure aluminum foil is subjected to chemical or electrochemical etching in an acidic solution to enlarge the surface, followed by chemical conversion in an aqueous solution of ammonium adipate, boric acid, phosphoric acid, etc. And an aluminum oxide film layer formed on the surface may be used.
  • the cathode foil a foil obtained by etching an aluminum foil having a purity of 99.9% and expanding the surface thereof may be used.
  • the cathode foil a foil obtained by forming a titanium nitride thin film on the surface of an etched aluminum foil (for example, described in Japanese Patent Application Laid-Open No. Hei 9-186504) may be used.
  • the electrolytic solution according to the present invention is impregnated into the separator of the capacitor element configured as described above.
  • the element impregnated with this electrolyte solution was stored in a bottomed cylindrical aluminum outer case, and a butyl rubber sealing member was inserted into the open end of the outer case. By drawing the end of the outer case and sealing the electrolytic capacitor, an aluminum electrolytic capacitor can be obtained. It is more preferable to coat the surface of the sealing body with a resin such as Teflon or to attach a plate such as a bakelite since the permeability of solvent vapor + is reduced. .
  • the butyl rubber used for the sealing body is composed of raw rubber composed of a copolymer of isoptylene and isoprene, a reinforcing agent (such as Rikibon black), a bulking agent (such as clay, talc, and calcium carbonate), and a processing aid (such as stearic acid, After adding and kneading a zinc oxide or the like, a vulcanizing agent, and the like, a rolled or molded rubber elastic body can be used.
  • a reinforcing agent such as Rikibon black
  • a bulking agent such as clay, talc, and calcium carbonate
  • a processing aid such as stearic acid
  • Vulcanizing agents include alkylphenol formalin resins; peroxides (dicumylperoxide, 1,1-DG (t-butylperoxy)) — 3,3,5-trimethylcyclohexane, 2,5-dimethyl-2,5- Di- (t-butylperoxy) hexane, etc.); quinoids (p-quinonedioxime, p, p'dibenzoylquinonedioxime, etc.);
  • the aluminum electrolytic capacitor of the present invention may have a hermetic seal structure or a structure hermetically sealed in a resin case (for example, described in Japanese Patent Application Laid-Open No. 8-148384).
  • a hermetic seal structure or a structure hermetically sealed in a resin case for example, described in Japanese Patent Application Laid-Open No. 8-148384.
  • the gas permeates through the rubber to some extent, so that the solvent evaporates from the inside of the capacitor to the atmosphere in a high-temperature environment, and from the air in a high-temperature, high-humidity environment. Moisture enters inside. Under these harsh environments, capacitors can experience undesirable changes in properties, such as reduced capacitance.
  • capacitors with a hermetically sealed structure or a structure sealed in a resin case exhibit stable characteristics even under the above-mentioned harsh environment because the amount of gas permeation is extremely small.
  • a second aspect of the present invention is an electrolytic solution for an electrolytic capacitor containing a salt and a solvent, wherein the electric conductivity X (mScnf 1 ) at 25 ° C. and the withstand voltage Y (V) of the capacitor are represented by the following formula: (I):
  • the electric conductivity X in the formula (I) is the electric conductivity of the electrolyte at 25 ° C; X
  • the electric conductivity X is preferably 4 mS ⁇ cm— 1 or more, and S mS 'cuT 1 or more. It is more preferable to use an electrolytic solution having a high electric conductivity, because an electrolytic capacitor having a lower impedance and a lower equivalent series resistance can be obtained. mS ⁇ cm- 1 .
  • the withstand voltage Y in the formula (I) is the withstand voltage of the electrolytic capacitor, and is a rising voltage for one hour when a constant current is applied to the electrolytic capacitor. It is defined as the voltage value at which spike or scintillation is observed
  • the method of measuring the withstand voltage Y in the present invention is as follows.
  • a winding type capacitor element (for a rated voltage of 200 V and a capacitance of 20 nF) is used as the aluminum electrolytic capacitor element (Fig. 1). After the wound type element is impregnated with the electrolytic solution, the aluminum electrolytic capacitor is housed in an aluminum outer case and sealed with butyl rubber vulcanized with peroxide to produce an aluminum electrolytic capacitor (FIG. 2). The withstand voltage Y is measured by applying a constant current of 10 mA to this capacitor at 125 and measuring the voltage-hour curve.
  • the withstand voltage Y is more than 0 V, preferably 50 V or more, and more preferably 100 V or more.
  • the upper limit is preferably as high as possible, but is usually about 300 V.
  • the combination of the salt and the solvent contained in the electrolytic solution of the present invention is not limited as long as the above formula (I) is satisfied.
  • the salt is tetrafluoroaluminate (eg, quaternary onium salt of tetrafluoroaluminic acid, amine salt, ammonium salt And a combination of these tetrafluoroaluminates with hydrogen phthalate, hydrogen maleate, and the like
  • the solvent is a carbonate, carboxylate, or phosphoric acid.
  • esters, nitriles, amides, sulfones, alcohols and water are selected from the group consisting of esters, nitriles, amides, sulfones, alcohols and water.
  • the tetrafluoroaluminate is a salt in which the anion component is a tetrafluoroaluminate ion as described in the first embodiment.
  • the anion component is a tetrafluoroaluminate ion as described in the first embodiment.
  • Specific examples thereof include quaternary ammonium salts, amine salts, ammonium salts and metal salts of tetrafluoroaluminic acid.
  • Specific examples and preferred examples of the cation component of these salts are given below. Are those described for the first aspect.
  • a tetrafluoroaluminate When a tetrafluoroaluminate is used, it may contain other than tetrafluoroaluminate ion as an anion component, and specific examples thereof include those described in the first embodiment.
  • the tetrafluoroaluminate ion in the anion component is preferably from 5 to 100 mol%, more preferably from 30 to 100 mol%, and particularly preferably from 50 to 100 mol%. And most preferably 100 mol%.
  • tetrafluoroaluminate is used in combination with hydrogen phthalate, hydrogen maleate, or the like as the salt, it is preferable that tetrafluoroaluminate is mainly used, and tetrafluoroaluminate is used based on the total weight of the salt.
  • the content of the aluminate is preferably 50% by weight or more, more preferably 60% by weight or more, further preferably 70% by weight or more, and the higher the ratio, the more preferable.
  • the preferred concentration of the salt used in the electrolytic solution of the present invention is preferably 5 to 40% by weight, and more preferably 10 to 35% by weight.
  • concentration the higher the withstand voltage of the electrolytic solution. Since there is a tendency to increase, the optimum concentration may be determined according to the rated voltage of the desired capacitor.
  • the salt when used in an electrolytic capacitor, the salt needs to be of high purity, so the salt is used after being purified to a desired purity by recrystallization or solvent extraction as necessary.
  • examples of the solvent include one or more selected from a carbonate, a carboxylate, a phosphate, a nitrile, an amide, a sulfone, an alcohol, and water. Illustrated in one embodiment Is included.
  • the solvent in the electrolytic solution is preferably 50% by weight or more, and from the viewpoint of safety, it is preferable that the solvent contains a nonaqueous solvent having a flash point of 70 ° C or more.
  • the electrolytic solution of the second embodiment of the present invention is more preferable in view of the characteristics of the electrolytic capacitor, when the main component of the solvent is a high-boiling solvent group, and when the main component of the solvent is a low-boiling solvent. If the group is divided into two.
  • the main component of the solvent is a group of high-boiling solvents
  • a high-boiling solvent group (boiling point of 250 ° C or more, melting point of 60 to 4).
  • dielectric constant ( ⁇ , 25 ° C) 25 or more low boiling point solvent group (boiling point 190 ° C or more, less than 250, melting point-60 to 40, and dielectric constant ( ( ⁇ , 25 ° C)
  • the weight ratio of the solvent belonging to the high boiling solvent group is equal to or greater than the weight ratio of the solvent belonging to the low boiling solvent group .
  • the main component of the solvent is a low-boiling solvent group means that the weight ratio of the solvent belonging to the low-boiling solvent group exceeds the weight ratio of the solvent belonging to the high-boiling solvent.
  • the solvent mainly belongs to either the high-boiling solvent group or the low-boiling solvent group, and the other solvents that do not belong to any of them are present as minor components. 0% by weight or less.
  • the electrolytic solution contains 50% by weight or more of a solvent, and the main component of the solvent is a group of high-boiling solvents (boiling point of 250 or more, melting point of 60 to 40 ° C , And dielectric constant ( ⁇ , 25 ° C.) 25 or more), an electrolytic capacitor having particularly excellent thermal stability can be obtained by using this electrolytic solution.
  • solvents belonging to the high-boiling-point solvent group account for 60% by weight or less based on the total weight of the solvent. It is preferably above, more preferably 70% by weight or more, particularly preferably 100% by weight.
  • Examples of the solvent used for such an electrolyte include sulfone, and particularly preferred are sulfolane and 3-methylsulfolane.
  • the electrolytic solution contains 50% by weight or more of a solvent, and the main component of the solvent is a group of low-boiling solvents (boiling point of 190 or more, less than 250 ° C, melting point of 16 ° C). 0 to 4 0 ° C, and dielectric constant if ( ⁇ , 2 5 ° C) 2 5 or more) belonging, by using this electrolytic solution, the electrolysis of c low impedance which can obtain particularly low impedance electrolytic capacitor From the viewpoint of obtaining a capacitor, the solvent belonging to the low boiling point solvent group is preferably at least 60% by weight, more preferably at least 70% by weight, particularly preferably at least 10% by weight, based on the total weight of the solvent. 0% by weight.
  • This electrolyte has the formula (II I):
  • Examples of the main component of the solvent used in such an electrolytic solution include one or more selected from the group consisting of carbonates, carbonates, phosphates, nitriles, amides and alcohols. Particularly preferred are lactone lactone and ethylene glycol.
  • a particularly preferable combination of a salt and a solvent is a salt.
  • the salt is tetraethylaluminate 1-ethyl-2,3-dimethylimidazolidinum or tetrafluoroaluminate 1,2,3,4-tetramethylimidazolinium
  • the solvent is r-butyrolactone.
  • a solvent using a combination of sulfolane and arptyrolactone is also preferable.
  • additives other than salts and solvents may be used in the electrolyte solution of the present invention.
  • Specific examples and preferable examples of the additive and the amount of the additive include those described in the first embodiment.
  • the measurement of the electric conductivity and the withstand voltage is a value measured for a stock solution containing no salt and a solvent without such an additive. If the stock solution satisfies the relationship represented by the formula (1), (II) or (III), and if necessary, further additives may be included in the scope of the present invention.
  • the life characteristics of a capacitor using such an electrolytic solution are more stabilized by controlling the water content.
  • the control of the water content is as described in the first embodiment.
  • the present invention also provides an electrolytic capacitor using the electrolytic solution of the second aspect.
  • the manufacturing method and components of the electrolytic capacitor are as described in the first embodiment.
  • Example 1 an electrolytic solution having a concentration of 25% by weight was prepared by dissolving the above-obtained triethylmethylammonium tetrafluoroaluminate in arbutyrolactone. The electrical conductivity (25 ° C.) of the electrolyte solution of Example 1 was measured immediately after preparation and after a heating test at 125 was performed for 25 hours.
  • an aluminum electrolytic capacitor having a structure in which the wound element shown in FIG. 1 is impregnated with an electrolytic solution, the wound element is housed in an aluminum outer case, and sealed with butyl rubber vulcanized with peroxide. Fabricated (Fig. 2).
  • ⁇ 3 ⁇ 4 ⁇ is 1-ethyl-2,3-dimethylimidazolinium ion
  • PH "" represents hydrogen fluoride. Comparing the example with the comparative example, it can be seen that the electrical conductivity of the example 1 is about twice as high as that of the comparative example, and that the change after heating is small and the thermal stability is excellent. Also, the withstand voltage is 2.5 to 3 times higher than that of the comparative example. (3) Other embodiments
  • the components were mixed according to the composition shown in Table 2 below to prepare an electrolytic solution.
  • the amount of each component is shown in parts by weight.
  • the obtained electrolytic solution was evaluated for electric conductivity and withstand voltage. First, the electrical conductivity at 25 ° C was measured. Next, the withstand voltage at 125 ° C. was measured in the same manner as in Example 1. —These results are shown in Table 2.
  • Table 2 Table 2
  • PH— is hydrogen phthalate ion, EDMH or 1-ethyl-2,3-dimethyl
  • the electrolytic solution of the present invention is preferable for an aluminum electrolytic capacitor for any use for low impedance grade and high rated voltage.
  • each component was mixed with the composition shown in Table 3 to prepare an electrolytic solution.
  • the amount of each component is shown in parts by weight.
  • Silica has an average particle size of about A 25 nm ethylene glycol sol was used.
  • 1-ethyl-2,3-dimethylimidazolinium tetrafluoroaluminate used in Examples 3 to 8
  • the same parts by weight of 1-ethyl-2,3-dimethylimidazonium hydrogen phthalate were used.
  • Example 9 Example 10 Example 11 Example 12 Example 13 Example 14 1-Ethyl tetrafluoroaluminate
  • the electrolytic solution of the present invention is suitable for aluminum electrolytic capacitors used for both low impedance grades and high rated voltages. .
  • an aluminum electrolytic capacitor having a rated voltage of 100 V and a capacitance of 56 / iF was produced using the electrolytic solutions of Examples 1, 3 and 4 described above. Further, as Example 15, an electrolytic solution obtained by further adding 3% by weight of water to a solution of 25% by weight of 1-ethyl-2,3-dimethylimidazolinium tetrafluoroaluminate in abutyrolactone solution was used. An aluminum electrolytic capacitor was prepared in the same manner as described above. The water content in the electrolytic solution used in Example 3 was measured by a Karl Fischer moisture meter and found to be 1% by weight. The capacitance at 120 Hz and the equivalent direct resistance (ESR) at 100 kHz were measured.
  • ESR equivalent direct resistance
  • Example 1 Example 3 Example 4 Example 15 Capacitance 1 ⁇ 54.8 54.8 54.8 54.5 Capacitance (after no-load test) 1 ⁇ ? 55.9 53.7 55.2 38.4 Equivalent series resistance /. ⁇ 0.0066 0.0063 0.0105 0.0073 Equivalent series resistance (after no-load test) / ⁇ 0.0067 0.0063 0.0107 0.0545 Appearance (after no-load test) Sealing swelling No change No change Sealing swelling Table 4 shows that the capacitors using the electrolytes of Comparative Examples 1, 5, and 6 could not be manufactured due to insufficient withstand voltage, whereas the capacitors of Examples 1, 3, 4, and 15 could not be manufactured. Using the liquid, a capacitor with good device characteristics could be manufactured.
  • the capacitors using the electrolytes of Examples 1, 3, and 4 showed almost no change in device characteristics after the no-load test, indicating that the capacitors had excellent thermal stability.
  • the appearance in the capacitors using the electrolytes of Examples 1 and 15, swelling was observed only in the sealing rubber part, suggesting that gas was generated inside the capacitors. It was found that such a capacitor using the electrolytic solution did not have such swelling and had better thermal stability.
  • an electrolytic solution for an electrolytic capacitor having high electric conductivity, excellent thermal stability, and high withstand voltage can be obtained. Also, by using this electrolytic solution for an electrolytic capacitor, an electrochemical device having low impedance, excellent thermal stability and high withstand voltage can be obtained.

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  • Electric Double-Layer Capacitors Or The Like (AREA)
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Abstract

La présente invention concerne une solution électrolytique pour un condensateur électrolytique d'électro-conductivité élevée, d'excellente stabilité thermique et de haute tension de résistance. L'invention concerne plus particulièrement une solution électrolytique destinée à un condensateur électrolytique se caractérisant en ce qu'il contient des ions tétrafluoroaluminate. L'invention concerne aussi une solution électrolytique pour un condensateur électrolytique contenant un sel et un solvant, caractérisée en ce que l'électroconductivité X (mS.cm-1) à 25 °C et que la tension de résistance Y (V) d'un condensateur respecte les relations Y ≥ 7,X + 150 dans l'expression (I) et X ≥ 4, Y > 0.
PCT/JP2002/004571 2001-05-11 2002-05-10 Solution electrolytique pour condensateur electrolytique et condensateur electrolytique utilisant cette solution WO2002101773A1 (fr)

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EP02778902A EP1394824A4 (fr) 2001-05-11 2002-05-10 Solution electrolytique pour condensateur electrolytique et condensateur electrolytique utilisant cette solution
CNB028097165A CN100394522C (zh) 2001-05-11 2002-05-10 电解电容器用电解液及使用该电解液的电解电容器
US10/704,803 US7072173B2 (en) 2001-05-11 2003-11-12 Electrolyte for electrolytic capacitor and electrolytic capacitor using the same
US11/304,600 US7460357B2 (en) 2001-05-11 2005-12-16 Electrolyte for electrolytic capacitor and electrolytic capacitor using the same

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CN101261900B (zh) 2011-02-02
CN1511327A (zh) 2004-07-07
JP2009161537A (ja) 2009-07-23
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US7460357B2 (en) 2008-12-02
US20040095708A1 (en) 2004-05-20
JP2011181956A (ja) 2011-09-15
US20060092597A1 (en) 2006-05-04
EP1394824A1 (fr) 2004-03-03
US7072173B2 (en) 2006-07-04
JP4631975B2 (ja) 2011-02-16
CN101261900A (zh) 2008-09-10
JP2009239291A (ja) 2009-10-15
CN100394522C (zh) 2008-06-11

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